Ammonia synthesis autoclave



- E. H. ARNOLD ET fain AMMONIA SYNTHESIS AUTOGLMEv Filed Nov'. y9. .1.921

ATTORNEY' v HR.'

- WEEE Patented July 3l, i923.

earner Aortica.'

EDWIN H. ARNOLD, F COVENTRY, AND WILLIAM T. WAKEFORD, OF PROVIDENCEX RHODE ISLAND, ASSIGNORS TO THE NITROGEN CORPORATION, OF .PROVIDENCEf RHODE ISLAND, CORPORATION 0F RHODE ISLAND. l

AMMONIA SYNTHESIS AUTOCLAVE.

Application filed November 9, 1921. Serial No. 514,088.

ToaZZ whom t may concern;

Be it known that we, EDWIN H. ARNOLD and `WILLIAM T. VVAKEFORD, citizens of the United States, residing at Coventry and' Providence, lin the counties of Kent and Providence, respectively, and State of Rhode lsland, have invented certain new and uscful Improvements' in Ammonia Synthesis Autoclaves, of which the following is 'a specification.

This invention relates to an improved ammonia synthesis autoclave and more particularly to certain improvements therein whereby the manipulation of thc salue for the removal and insertion of the charge may be facilitated with consequent saving of time and labor, and increased eticiency obtained by preventing leakage under high pressures and temperatures.

One object of the invention is to provide a device of this character having an improved form of closure whereby the same may e readilyopened or closed without undue y loss of time and at the same time provide. a

closure which will prevent the escape of the gases and'not become Warped or distorted under the rconditions of temperature and pressure required in devices of this character. y

Another object of thevinvention is to provide a device of this character which will lend itself readily to the operations of removing the spent charge and replacing the same wit-h another without the expcruftiturc of unnecessary time and labor.

Another object of the invention is to proi vide a device of this character which is s o v constructed and arranged as to withstand highl temperatures. and pressures without danger of leakage and wherein the several parts are so connected together and arranged relative to each other as to combine high efficiency of operation with simplicity of construction Whereb 'the danger of explosions or injuryto t e apparatus or the attendants will be reduced to a minimum.y

vOther obiccts and advantages of the invention relate to certainimproved details of construction and modes of operation as will be more fully set forth in the detailed description to fcllo v Referring to the drawings:

Fig. l is a perspective view of the autoclave in its operating position, the insulation container surrounding the same being shown in section to better illustrate the autoclave and its associated parts. y y

Fig. `2 is an enlarged vertical sectional of the autoclave showing the construct-ion of the closure.

Fig. l3 is an enlarged detail sectional view of the pressure plate and open end ot the autoclave showing the manner of positioning the parts relative toeach other and the packinginterposed therebetween.

Fig. 4 is a vertical sectional view of the upper' end of the autoclave showing a slightly modified form of the invention, and,

Fig. 5 is a top plan view ofthe structure shown in Fig. 4.

In the embodiment of the mvontion illustrated herewith 1. designates a container which may be rectangular or of any other suitable shape Within which is enclosed the view taken through the upper reduced end I autoclave 2 surrounded by suitable iusulating material 3, such as kieselguhr, whereby the temperature of the autoclave may be suitably maintained without undue loss by reason of radiation. y

The autoclave 2 is provided with an elongated body,portion 4 and upper and lower reduced end portions 5 and 6 respectively.

. with another. The form an of the openings in the ends of the -autoclave closed lower end 10, is also inserted throu h the 'wall otr the autoclave, being preferab y welded: thereto at its point ot entry, and extends to a point near the lower end of the autoclave. The tube 9 serves as a container for an electric pyroxneter 11 of standard construction from which extend connecting wires 12 and 13 for registering the temperature of the interior of the autoclave.

The autoclave is located in substantially upright position as show-n in Fig. 1 of the drawings, and the reduced ends are provided with openings for the removal and inscrtion of the charges, each oi these ends being provided with closures of a character adapted to withstand high temperatures and pressures without danger of leakage while at the Sametime being so .constructed as to permit 'the ready removal and replacement of the closures whenv it becomes necessary to renuove the spent charge and re lace the saine arrangement and the closure elements for closing the same are' similar at both ends of the autoclave and one of these is shown in detail in Fig 2 of the drawings. l

The reduced open end 5 of the autoclave is provided with 'an exterior threaded portion 15 upon which is threaded 'a cupshaped cap lt, within the base portion o which is threaded a pressure screw 17 of fairly Alarge dimensions relative to the size of the opening in the end of the autoclave. rll`he screw 12 is provided with an angular head 18 whereby the same may be rotated in the `cap 1d and the pressure screw -is so ositioned that its airis corresponds substannally with the major asis of the autoclave. A ressure plate 19 fits over the open end of t e autoclave within the cap i6 and is provided upon the side adjacent to the screw 1'? with a seat 20 against which the end or1 the screw may press when forced thereagainst.

V-shaped grooves 21 an 22 are-formed upon the annular face prese ted by the open end of the autoclave and the opposed tace of the pressure plate respectively, these grooves being of similar sizp and shape and arranged to register with a'ch other when the pressure late is posiii'oned over the open end of t e autoclaveiand within the cap 16. A packing ring7 23 is interposed between the annular face of the open end of the autoclave and the pressure plate 16 to fit within the registering grooves 21 and 22. and sheets of packing material .2t and 25 of asbestos, suitable metal or other appro priate Amaterial. are preferably placed upon each. side of the ring 23between the ring and the-end of the autoclave and the pres! sure plate respectively.

- lin a plying the closure elements to the ends o the autoclave the ring 23 and packing'strips 2d and 25 are placed over the open Messen end of the autoclave and the pressureplate 19 then placed in position sovthat the ring v down the desired distance. The screw 17 is y then rotated to bring the end thereo into contact with the seat 20 and force the pressure plate towards the open end o the autoclave whereby the pressure plate and packing are forced firmly against the annular face oi' the open end and into such close engage ment as to prevent leakage oi gases through the closure elements.

ln Fi s. 4; and 5 of the drawings is shown a slight y niodiiied forni o' the invention wherein the tube 9 having a closed lower end 10 for containing the pyrometer 1l is inserted through the pressure plateltl and the cap 16 substantially centrally thereof instead of bein@r passed through the wall of the autoclave. ln this case it is preferred to pass the tube through an opening 30 formed substantially centrally of the cap 16 to permit movement of the cap relative to the tube, while the tube 9 is welded to the pressure plate 19 where it passes therethrough. By this arrangement of the parts the tubs and pressure plate are removable and replaceable as a unit while the cap may be positioned over the pressure plate and tube after the same have been placed in position. The annular face of the open end oil the autoclave and the ressure plate are provided with registering L.grooves 2l and. 22

.for the reception of a packing ring 23 and packing sheets 24C and 25 as in the iorrn previously described.

1in this form of the invention a plurality .L

yly against the upper face of the pressure plates.

lln devices of this character as heretofore employed Where .temperatures oi 400 to 600O C are employed and the being synthesized are subjected to high pressures ofV from 1000 to 1500 pounds per square inch great difiiculty has been encountered in providing a closure 'for the autoclave which will withstand temperatures and pressures of the orders mentioned without becoming warped or distorted so as to malte the taslr ot removing; and repliseingn tlie'sarne eir-1 treinely difficult aswell as in eases causing loss of the tov si 'i es to naal-re it necessary stepl operations and repair; the parts. 'Ey the use the struc- Bil ture shown and described herewith these difficulties have been overcome and the expenditure of time and labor in removing and replacing the closures greatly reduced es well as the danger of leakage substantiall eliminated. In the use of our improve structure important economles of operation are effected by the provision of the novel closures andV the arrangement of the parts. It has heretofore been the practice to use an autoclave provided with a single opening positioned at the-top thereof and in removing a chargeit was therefore necessary to remove the closure and force the spent material out by forcing the Working gases into the autocalve under high pressures through the pipes 7 and 8. This is a long and difficult procedure but was the onlyy practicable method so long as no approximately perfect closure mechanism could be provided for the openings in the autoclave, since to provide another opening in the autocalve would double the losses from leakage as well as increase the time and labor in removing and replacing the closures. ByV means -of our improved construction ofclosure iWe are enabled to provide openings' both at the top and at the bottom of the autoclave wherebyin the removal of the spent charge' the bottom closure may be. removed Without disturbing the top closure, and the material forced out by the combined action o-'I grav' ity and gas pressure introduced through one of the pipes 7 and 8. Upon the removal of' the charge the closure at the bottom of the autoclave is replaced and that at the top opened through which a fresh charge is insorted. Thus it will be seen that important advantages of operation are secured as well as a more'eflicient closure mechanisinfor devices of this character. The autoclave as well as the cap pressure plate and packing ring are preferablyA all formedof steel, vanadiuni steel alloy or other suitable alloy, the autoclave being of seamless construction to better withstand the pressures employed. VVhileo we have shown and described in considerable detail one embodiment of o ur invention which We have found efficient in operation', We are aware that various modificattions may be made therein without departing from the spirit of our invention, and therefore, We do not desire to be limited to the precise details of construction shown and described except as the same may properly be included Within the scope of the appended claims when broadly construed.

Having described our invention, what We claim is: i

1. An ammonia synthesis autoclave comprising an elongated body portion provided With reduced ends, inlet and'outlet pipes entering said body portion and terminating-at. unequal-distances from the base thereof, a tube provided with a closed end4 projecting within said body portion, and independently removable closures for the reduced ends of said body portion.

2. An ammonia synthesis autoclave comprising an elongated body portion formed of a single metallic shell surrounded by heat' insulating material and having inlet and outlet pipes projecting therein for con- Veying gasesto and from said body portion, said body portion being .provided with reduced ends, and yindependently removable closures for said reduced ends.

3. An ammonia synthesis autoclave comprising a Ybody portion provided with a reduced open end, a cap threaded upon the reduced end of the autoclave and providedA with a threaded opening, a closure plate fitting over the'open end of the autoclave and'within the cap, vand a pressure. sc-'rew threaded Within the threaded opeingdn the cap and bearing againstone side'ol the pressure plate to hold the same firmly in contact with the open end of the autoclave. l 4. An ammonia synthesis autoclave comprising a body portion provided with a re- -gduc'ed open end, a closure for said open end :comprising a cap threaded upon the reduced end of the autoclave, a pressure plate positioned within the cap and contacting with the open end of the reduced end of the autoclave, andl adjustable means carried by the cap for exerting pressure upon the pressure plate and holding the same firmly against the open end oflthe autoclave.

5. An ammonia synthesis autoclave comprising a seamless body portion provided with a reduced end, and a closure therefor comprising a pressure plate, a cap enclosing said plate and engaging the re.. duced end of said autoclave, and a means carried by said cap and ladjustable relative thereto for forcing said-platento close engagement with said reduced end and holding the same in position under pressure. y

6. In an ammonia synthesis autoclave comprising .a body portion provided with a reduced open end, a pressure plate fitting over said open end, a packing ring interposed between the end of said autoclave and said plate; a member secured to said autoclave and enclosing said plate, and adjustable means carried by said member for exerting pressure upon said plate to -force the same towards said reduced end.

7. ln an ammonia synthesis autoclave ,comprising a body portion provided with an open end, a pressure plate fitting over said open end the adjacent surfaces of said end` and said plate being provided with cooperating grooves. a packing ring interposed between theend of the autoclave and said plate in registry with said grooves, a membersecured' to theeutoclove and enclosing said plstepend sdjusteble vineens cerriedby seid member for; exerting pressure upon seid plete to. force vthe seme towards said opeiie'nd of :the autoclave. i

.8..An :ammonioJ synthesis 'autoclave comprising.. a loody .portion vdonned oie single metalhc shell vand provided with reduced ends, means for placing the interior of seid autoclave under pressure, and independently removable closures for the reduced ends of said Aautoclave whereby the charge may. be Withdrawn and replaced through the .closures located et oppositeends of the autoclave.

9. An `einiiioniel synthesis autoclave comprising e body portion formed of o single metallic shell provided with oppositelvY located openings, .means for placing the interior of said' autoclave under pressure, end independently/.removable closures for seid openings whereby the charge vmay be rei moved. from said autoclave bv the combined inuence of gravity end pressure.

,lG. lnenxammonia synthesis autoclave, e seamless -body portionl provided with an opeixfmgtherein, a, closure for seid opening, an Vinlet andoutlet pipe for said autoclave eachppening into the interior thereof e'nd 'eccesso terminated et e lower. level themseid oue? Jlet pipe, and e pyromemr eeciosing tube projecting Within seid body portion eind weldedthereto. y

iL A11 emmonie synthesis sutoclevie prol vided with eu open end, s pressure plete tittiug overseid openl end and serving es e closure therefor, -e csp detechebly cured. to the outer surface ofseid autoclave edjecent to seid open yeed, end indel l pendently edgustable meeriscerricd by seid oep for forcing seid pressure plete, tovverds the end of seid eutocleve end holding tic pressure plete securely 'tliereogeiiist l l2. lin ein ammonia synthesie'` autoclave comprising e body portion provided with e reduced open end, e pressure plete tted over seid open leind, e. member overlyiiiv, seid pressure plete-end secured tothe end portion oi" seid eutocleve end means cerried by seid member for exerting pressure upon seid pressure plete to force the some towards seid reduced cud, l

in testimony vliiereoi' We have eixed our signatures.

sowie ist esserlo, vviLLri-ivi vvsiocsoieio. 

